CN106833606B - A kind of titanate ability of reverse photochromism material and preparation method thereof - Google Patents
A kind of titanate ability of reverse photochromism material and preparation method thereof Download PDFInfo
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Abstract
The application belongs to inorganic photochromic function luminescent material technical field, and in particular to a kind of titanate ability of reverse photochromism material and preparation method thereof.Photochromic material provided by the present invention is Ba1‑xTi4O9:xRe；Wherein, Re is the rare earth element being doped in basis material, is Y, La, Ce, Pr, Nd, Sm, Gd, Tb, Dy, Ho, Er, Tm, Eu, Yb or Lu；X is the doping mole of Re, 0≤x≤0.1.Photochromic material of the present invention has the advantages that fatigue resistance is good, it is low that it prepares cost of material, it is not high to equipment requirement, preparation is simple, favorable repeatability, obtained product stability is high, can be widely applied to the fields such as optical information storage, light regulation, optical device materials, inductor, the photograph of anti-fake and autography holographic recording.
Description
Technical field
The invention belongs to inorganic photochromic function luminescent material technical fields, and in particular to a kind of titanate is reversible photic
Off-color material and preparation method thereof.
Background technique
Photochromism refers to compound after the irradiation by certain wavelength, and color can slowly become another face
Color after the irradiation again of another suitable wavelength, and can slowly restore to original color.People are to metachromatism
Research is more early, has found that the photochromism of inorganic compound and organic compound early in 19th-century people's forties.
Nineteen seventies, professor Heller etc., which proposes photochromic material, can be used for information storage and optical recording, cause
The great interest that people study photochromic material.Since photochromic material is in optical information storage, light regulation, optical device
The various fields such as material, anti-fake, decoration, inductor and radiation metering meter have potential application, inorganic photochromic material
The material also therefore concern by more and more people.
Past is concentrated mainly on organic photochromic material to photochromic material focus of attention and unorganic glass is photic
Off-color material field, and obtain sizable progress.From the point of view of existing literature and relevant report, about organic photochromic material
Synthesis, performance, mechanism with unorganic glass photochromic material and application comparative maturity.Organic compound has excellent
Molecule cuts the superiority with modification, but also has robustness, stability insufficient simultaneously, be easily oxidized degradation or even lose discolouration
The defect of energy.And inorganic photochromic material stability with higher, excellent fatigue resistance and formability, it just can be with
The deficiency of organic photochromic material is made up, there is very big application prospect.Some main inorganic light reported at present
Cause off-color material as follows: iron-containing SrTiO3And TiO2(Phys.Rev.Lett., Vol.21,1331, (1968)), BaMgSiO4:
Eu2+(Appl.Phys.Lett.,Vol.97,181905,(2010)),CaAl2O4: Eu2+,Nd3+(Opt.Mater.Express,
Vol.3,787,2013), ZnGa2O4: Bi3+(Opt.Mater.Express, Vol.2,1378, (2012)), Sr2SnO4: Eu3+
(Appl.Phys.Lett., Vol.102,031110, (2013)), Ba5(PO4)3Cl:Eu2+(J.Photochem.Photobiol
A,Vol.251,100,(2013)),Zn2GeO4:Eu2+(Mater.Lett., Vol.134,187, (2014)), Sr3YNa(PO4)3F:Eu2+(J.Mater.Chem.C.Vol.3,9435-9443(2015)),Na0.5Bi2.5Nb2O9:Re3+(Re=Sm, Pr, Er)
(ACS.Appl.Mater.Inter.,Vol.7,25289-25297(2015)),Mg8GaGe8O20:Cr3+
(J.Mater.Chem.C.Vol.4,6614-6625(2016)),Ba3MgSi2O8:Eu2+(J.Lumin.173,237-242
(2016)),MgGeO3:Yb3+(Light.Sci.Appl.Vol.5,e16124(2016)),Na0.5Bi4.5Ti4O15:Re3+(Re=
Sm, Pr, Er) (ACS.Appl.Mater.Inter., Vol.8,34581-34589 (2016)) etc..However, inorganic so far
But very slowly, type and color change are also extremely limited for the development speed of photochromic material, this largely upper limit
The application of inorganic photochromic material is made.Moreover, above-mentioned inorganic photochromic material is largely what divalent europium adulterated
Inorganic compound, preparation need under reducing atmosphere, the high requirements on the equipment and preparation difficulty.
Summary of the invention
In view of this, leading to the present invention provides a kind of novel titanate ability of reverse photochromism material and preparation method thereof
The a small amount of rare earth element of overdoping achievees the effect that its photochromic degree of adjustment, specific technical solution are as follows:
The present invention provides a kind of titanate ability of reverse photochromism materials, as shown in formula (I):
Ba1-xTi4O9:xRe (Ⅰ)；
Wherein, Re is rare earth element, in Y, La, Ce, Pr, Nd, Sm, Gd, Tb, Dy, Ho, Er, Tm, Eu, Yb and Lu
It is one or more；
X is the doping mole of Re, 0≤x≤0.1.
The present invention also provides a kind of preparation methods of above-mentioned titanate ability of reverse photochromism material, comprising:
Ba compound, compound containing Ti and the mixing of compound containing Re will be contained, be sintered, obtaining the titanate can backlight
Cause off-color material；
Wherein, Re is selected from one of Y, La, Ce, Pr, Nd, Sm, Gd, Tb, Dy, Ho, Er, Tm, Eu, Yb and Lu or more
Kind；
The molar ratio of Ba, Ti and Re are (1-x): 4:x in the compound containing Ba, compound containing Ti and compound containing Re；0
≤x≤0.1。
Preferably, the compound containing Ba be selected from one of oxide of the carbonate of Ba, the nitrate of Ba and Ba or
It is a variety of；
The compound containing Ti is selected from one of nitrate of the oxide of Ti, the carbonate of Ti and Ti or a variety of；
The compound containing Re is selected from the oxide of Re and/or the nitrate of Re.
Preferably, the temperature of the sintering is 1100~1400 DEG C.
Preferably, the time of the sintering is 3~6h.
Preferably, the atmosphere of the sintering is air atmosphere.
It preferably, further include pre-burning before the sintering；
The temperature of the pre-burning is 500~600 DEG C.
Preferably, the time of the pre-burning is 2~3h.
The present invention provides a kind of novel titanate ability of reverse photochromism material, the expression formula of the photochromic material is
Ba1-xTi4O9:xRe；Wherein, Re is the rare earth element being doped in basis material, be Y, La, Ce, Pr, Nd, Sm, Gd, Tb, Dy,
Ho, Er, Tm, Eu, Yb or Lu；X is the doping mole of Re, 0≤x≤0.1.The present invention regulates and controls light by adjusting the doping of Re
The discoloration for causing off-color material obtains a kind of inorganic ability of reverse photochromism material, under the irradiation of ultraviolet light its color by
White becomes pink, can revert to white again after sunlight irradiates or is heat-treated, have the advantages that fatigue resistance is good.Together
When, it is low to prepare cost of material, and preparation is not necessarily to reducing atmosphere, and not high to equipment requirement, preparation is simple, repeatability
Good, obtained product stability is high, can be widely applied to optical information storage, light regulation, optical device materials, inductor, it is anti-fake,
The fields such as the photograph of autography holographic recording, decoration, radiation metering meter and protective packaging material.
Detailed description of the invention
In order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, to embodiment or will show below
There is attached drawing needed in technical description to be briefly described, it should be apparent that, the accompanying drawings in the following description is only this
The embodiment of invention for those of ordinary skill in the art without creative efforts, can also basis
The attached drawing of offer obtains other attached drawings.
Fig. 1 is non-impurity-doped BaTi prepared in embodiment 14O9Photochromic material is handed over by ultraviolet light and visible light
For the diffusing reflectance spectra after irradiation；
Fig. 2 is Eu prepared in embodiment 23+The BaTi of doping4O9Photochromic material is by ultraviolet light and visible
Diffusing reflectance spectra after light alternating irradiation；
Fig. 3 is Sm prepared in embodiment 33+The BaTi of doping4O9Photochromic material is by ultraviolet light and visible
Diffusing reflectance spectra after light alternating irradiation；
Fig. 4 is Ce prepared in embodiment 43+The BaTi of doping4O9Photochromic material is by ultraviolet light and visible
Diffusing reflectance spectra after light alternating irradiation；
Fig. 5 is Tb prepared in embodiment 53+The BaTi of doping4O9Photochromic material is by ultraviolet light and visible
Diffusing reflectance spectra after light alternating irradiation；
Fig. 6 is Pr prepared in embodiment 63+The BaTi of doping4O9Photochromic material is by ultraviolet light and visible
Diffusing reflectance spectra after light alternating irradiation；
Fig. 7 is Er prepared in embodiment 73+The BaTi of doping4O9Photochromic material is by ultraviolet light and visible
Diffusing reflectance spectra after light alternating irradiation；
Fig. 8 is Nd prepared in embodiment 83+The BaTi of doping4O9Photochromic material is by ultraviolet light and visible
Diffusing reflectance spectra after light alternating irradiation；
Fig. 9 is Yb prepared in embodiment 93+The BaTi of doping4O9Photochromic material is by ultraviolet light and visible
Diffusing reflectance spectra after light alternating irradiation；
Figure 10 is Tm prepared in embodiment 103+The BaTi of doping4O9Photochromic material is by ultraviolet light and can
Diffusing reflectance spectra after light-exposed alternately irradiation.
Specific embodiment
The present invention provides a kind of titanate ability of reverse photochromism materials, as shown in formula (I):
Ba1-xTi4O9:xRe (Ⅰ)；
Wherein, Re is rare earth element, in Y, La, Ce, Pr, Nd, Sm, Gd, Tb, Dy, Ho, Er, Tm, Eu, Yb and Lu
It is one or more；
X be Re doping mole, 0≤x≤0.1, preferably 0.01≤x≤0.08, more preferably 0.02≤x≤
0.07, most preferably x=0.005.
The present invention also provides the preparation methods of above-mentioned titanate ability of reverse photochromism material, comprising:
Ba compound, compound containing Ti and the mixing of compound containing Re will be contained, be sintered, obtaining the titanate can backlight
Cause off-color material；
Re is selected from one of Y, La, Ce, Pr, Nd, Sm, Gd, Tb, Dy, Ho, Er, Tm, Eu, Yb and Lu or a variety of；
In the compound containing Ba, compound containing Ti and compound containing Re the molar ratio of Ba, Ti and Re be (1-x): 4:x, 0
≤x≤0.1；Most preferably 0.995:4:0.005.
The present invention is not particularly limited the source for preparing raw material, is commercially available.In the present invention, contain Ba
Compound is preferably one of oxide of the carbonate of Ba, the nitrate of Ba and Ba or a variety of, most preferably BaCO3；Contain
Ti compound is preferably one of nitrate of the oxide of Ti, the carbonate of Ti and Ti or a variety of, most preferably TiO2；Contain
Re compound is preferably the oxide of Re and/or the nitrate of Re, the most preferably oxide of Re.
Further, the temperature of the sintering is 1100~1400 DEG C, and the time is 3~6h.
Further, the atmosphere of the sintering is air atmosphere.
The present invention does not make special limitation to the equipment of the sintering, using the normal sintering equipment of those skilled in the art
?.In embodiments of the present invention, it is sintered using high temperature process furnances or Muffle furnace.
It further, further include pre-burning before the sintering, the temperature of the pre-burning is preferably 500~600 DEG C, soaking time
Preferably 2~3h.
Technical solution of the present invention is clearly and completely described below in conjunction with the specific embodiment of the invention, it is clear that
Described embodiment is a part of the embodiment of the present invention, instead of all the embodiments.Those skilled in the art should manage
Solution, modifies to specific embodiments of the present invention or is replaced on an equal basis to some technical characteristics, without departing from the present invention
The spirit of technical solution should all cover in the scope of protection of the invention.
Embodiment 1
According to expression formula BaTi4O9, BaCO is weighed respectively3(analysis is pure) and TiO2(spectroscopic pure), molar ratio 1:4,
It is sufficiently mixed and is put into corundum crucible after being ground to uniformly, high temperature process furnances are then put into, at 1250 DEG C in air environment
Calcination 5h finally regrinds to powder with taking-up sample after furnace cooled to room temperature, obtains the titanate of white powder
Ability of reverse photochromism material.
Titanate ability of reverse photochromism material obtained in the present embodiment is divided using ultraviolet-visible spectrophotometer
Analysis obtains its spectrogram that diffuses after ultraviolet light and visible light alternately irradiate, as shown in Figure 1, Fig. 1 shows that the material exists
The ability of reverse photochromism phenomenon that ultraviolet light and visible light generate after alternately irradiating, this reversible process repeatability are high.The present embodiment
The BaTi of preparation4O9After 254nm ultraviolet excitation, color is faded to greyish black non-impurity-doped photochromic material by white
Color, color is gradually recovered again as original white after sunlight irradiates.
Embodiment 2
According to expression formula Ba0.995Ti4O9:0.005Eu3+, BaCO is weighed respectively3(analysis is pure), TiO2(analysis pure) and
Er2O3(spectroscopic pure), molar ratio 0.995:4:0.005 are sufficiently mixed and are put into corundum crucible after being ground to uniformly,
Then high temperature process furnances are put into, the calcination 5h in air environment at 1250 DEG C, finally with taking out sample after furnace cooled to room temperature
Product are regrind to powder, obtain the titanate ability of reverse photochromism material of white powder.
Titanate ability of reverse photochromism material obtained in the present embodiment is divided using ultraviolet-visible spectrophotometer
Analysis obtains its spectrogram that diffuses after ultraviolet light and visible light alternately irradiate, as shown in Fig. 2, Fig. 2 shows that the material exists
The ability of reverse photochromism phenomenon that ultraviolet light and visible light generate after alternately irradiating, this reversible process repeatability are high.The present embodiment
The Ba of preparation0.995Ti4O9:0.005Eu3+Photochromic material is after 254nm ultraviolet excitation, and color is by white gradual change
For grey black, color is gradually recovered again as original white after sunlight irradiates.Trivalent europium ion is used in the present embodiment
Doped titanic acid base status improves photochromic properties, and reducing atmosphere is not necessarily in preparation process, low for equipment requirements, preparation process letter
It is single easy.
Embodiment 3
According to expression formula Ba0.995Ti4O9:0.005Sm3+, BaCO is weighed respectively3(analysis is pure), TiO2(analysis pure) and
Sm2O3(spectroscopic pure), molar ratio 0.995:4:0.005 are sufficiently mixed and are put into corundum crucible after being ground to uniformly,
Then high temperature process furnances are put into, the calcination 5h in air environment at 1250 DEG C, finally with taking out sample after furnace cooled to room temperature
Product are regrind to powder, obtain the titanate ability of reverse photochromism material of white powder.
Titanate ability of reverse photochromism material obtained in the present embodiment is divided using ultraviolet-visible spectrophotometer
Analysis obtains its spectrogram that diffuses after ultraviolet light and visible light alternately irradiate, as shown in figure 3, Fig. 3 shows that the material exists
The ability of reverse photochromism phenomenon that ultraviolet light and visible light generate after alternately irradiating, this reversible process repeatability are high.The present embodiment
The Ba of preparation0.995Ti4O9:0.005Sm3+Photochromic material is after 254nm ultraviolet excitation, and color is by white gradual change
For grey black, color is gradually recovered again as original white after sunlight irradiates.
Embodiment 4
According to expression formula Ba0.995Ti4O9:0.005Ce3+, BaCO is weighed respectively3(analysis is pure), TiO2(analysis pure) and
Ce2O3(spectroscopic pure), molar ratio 0.995:4:0.005 are sufficiently mixed and are put into corundum crucible after being ground to uniformly,
Then high temperature process furnances are put into, the calcination 5h in air environment at 1250 DEG C, finally with taking out sample after furnace cooled to room temperature
Product are regrind to powder, obtain the titanate ability of reverse photochromism material of pale yellow powder shape.
Titanate ability of reverse photochromism material obtained in the present embodiment is divided using ultraviolet-visible spectrophotometer
Analysis obtains its spectrogram that diffuses after ultraviolet light and visible light alternately irradiate, as shown in figure 4, Fig. 4 shows that the material exists
The ability of reverse photochromism phenomenon that ultraviolet light and visible light generate after alternately irradiating, this reversible process repeatability are high.The present embodiment
The Ba of preparation0.995Ti4O9:0.005Ce3+Photochromic material is after 254nm ultraviolet excitation, and color is by white gradual change
For grey black, color is gradually recovered again as original white after sunlight irradiates.
Embodiment 5
According to expression formula Ba0.995Ti4O9:0.005Tb3+, BaCO is weighed respectively3(analysis is pure), TiO2(analysis pure) and
Tb4O7(spectroscopic pure), molar ratio 0.995:4:0.005 are sufficiently mixed and are put into corundum crucible after being ground to uniformly,
Then high temperature process furnances are put into, the calcination 5h in air environment at 1250 DEG C, finally with taking out sample after furnace cooled to room temperature
Product are regrind to powder, obtain the titanate ability of reverse photochromism material of pale yellow powder shape.
Titanate ability of reverse photochromism material obtained in the present embodiment is divided using ultraviolet-visible spectrophotometer
Analysis obtains its spectrogram that diffuses after ultraviolet light and visible light alternately irradiate, as shown in figure 5, Fig. 5 shows that the material exists
The ability of reverse photochromism phenomenon that ultraviolet light and visible light generate after alternately irradiating, this reversible process repeatability are high.The present embodiment
The Ba of preparation0.995Ti4O9:0.005Tb3+Photochromic material is after 254nm ultraviolet excitation, and color is by white gradual change
For grey black, color is gradually recovered again as original white after sunlight irradiates.
Embodiment 6
According to expression formula Ba0.995Ti4O9:0.005Pr3+, BaCO is weighed respectively3(analysis is pure), TiO2(analysis pure) and
Pr6O11(spectroscopic pure), molar ratio 0.995:4:0.005 are sufficiently mixed and are put into corundum crucible after being ground to uniformly,
Then high temperature process furnances are put into, the calcination 5h in air environment at 1250 DEG C, finally with taking out sample after furnace cooled to room temperature
Product are regrind to powder, obtain the titanate ability of reverse photochromism material of pale yellow powder shape.
Titanate ability of reverse photochromism material obtained in the present embodiment is divided using ultraviolet-visible spectrophotometer
Analysis obtains its spectrogram that diffuses after ultraviolet light and visible light alternately irradiate, as shown in fig. 6, Fig. 6 shows that the material exists
The ability of reverse photochromism phenomenon that ultraviolet light and visible light generate after alternately irradiating, this reversible process repeatability are high.The present embodiment
The Ba of preparation0.995Ti4O9:0.005Pr3+Photochromic material is after 254nm ultraviolet excitation, and color is by white gradual change
For grey black, color is gradually recovered again as original white after sunlight irradiates.
Embodiment 7
According to expression formula Ba0.995Ti4O9:0.005Er3+, BaCO is weighed respectively3(analysis is pure), TiO2(analysis pure) and
Er2O3(spectroscopic pure), molar ratio 0.995:4:0.005 are sufficiently mixed and are put into corundum crucible after being ground to uniformly,
Then high temperature process furnances are put into, the calcination 5h in air environment at 1250 DEG C, finally with taking out sample after furnace cooled to room temperature
Product are regrind to powder, obtain the titanate ability of reverse photochromism material of white powder.
Titanate ability of reverse photochromism material obtained in the present embodiment is divided using ultraviolet-visible spectrophotometer
Analysis obtains its spectrogram that diffuses after ultraviolet light and visible light alternately irradiate, as shown in fig. 7, Fig. 7 shows that the material exists
The ability of reverse photochromism phenomenon that ultraviolet light and visible light generate after alternately irradiating, this reversible process repeatability are high.The present embodiment
The Ba of preparation0.995Ti4O9:0.005Er3+Photochromic material is after 254nm ultraviolet excitation, and color is by white gradual change
For grey black, color is gradually recovered again as original white after sunlight irradiates.
Embodiment 8
According to expression formula Ba0.995Ti4O9:0.005Nd3+, BaCO is weighed respectively3(analysis is pure), TiO2(analysis pure) and
Nd2O3(spectroscopic pure), molar ratio 0.995:4:0.005 are sufficiently mixed and are put into corundum crucible after being ground to uniformly,
Then high temperature process furnances are put into, the calcination 5h in air environment at 1250 DEG C, finally with taking out sample after furnace cooled to room temperature
Product are regrind to powder, obtain the titanate ability of reverse photochromism material of white powder.
Titanate ability of reverse photochromism material obtained in the present embodiment is divided using ultraviolet-visible spectrophotometer
Analysis obtains its spectrogram that diffuses after ultraviolet light and visible light alternately irradiate, as shown in figure 8, Fig. 8 shows that the material exists
The ability of reverse photochromism phenomenon that ultraviolet light and visible light generate after alternately irradiating, this reversible process repeatability are high.The present embodiment
The Ba of preparation0.995Ti4O9:0.005Nd3+Photochromic material is after 254nm ultraviolet excitation, and color is by white gradual change
For grey black, color is gradually recovered again as original white after sunlight irradiates.
Embodiment 9
According to expression formula Ba0.995Ti4O9:0.005Yb3+, BaCO is weighed respectively3(analysis is pure), TiO2(analysis pure) and
Yb2O3(spectroscopic pure), molar ratio 0.995:4:0.005 are sufficiently mixed and are put into corundum crucible after being ground to uniformly,
Then high temperature process furnances are put into, the calcination 5h in air environment at 1250 DEG C, finally with taking out sample after furnace cooled to room temperature
Product are regrind to powder, obtain the titanate ability of reverse photochromism material of white powder.
Titanate ability of reverse photochromism material obtained in the present embodiment is divided using ultraviolet-visible spectrophotometer
Analysis obtains its spectrogram that diffuses after ultraviolet light and visible light alternately irradiate, as shown in figure 9, Fig. 9 shows that the material exists
The ability of reverse photochromism phenomenon that ultraviolet light and visible light generate after alternately irradiating, this reversible process repeatability are high.The present embodiment
The Ba of preparation0.995Ti4O9:0.005Yb3+Photochromic material is after 254nm ultraviolet excitation, and color is by white gradual change
For grey black, color is gradually recovered again as original white after sunlight irradiates.
Embodiment 10
According to expression formula Ba0.995Ti4O9:0.005Tm3+, BaCO is weighed respectively3(analysis is pure), TiO2(analysis pure) and
Tm2O3(spectroscopic pure), molar ratio 0.995:4:0.005 are sufficiently mixed and are put into corundum crucible after being ground to uniformly,
Then high temperature process furnances are put into, the calcination 5h in air environment at 1250 DEG C, finally with taking out sample after furnace cooled to room temperature
Product are regrind to powder, obtain the titanate ability of reverse photochromism material of white powder.
Titanate ability of reverse photochromism material obtained in the present embodiment is divided using ultraviolet-visible spectrophotometer
Analysis obtains its spectrogram that diffuses after ultraviolet light and visible light alternately irradiate, and as shown in Figure 10, Figure 10 shows the material
The ability of reverse photochromism phenomenon generated after ultraviolet light and visible light alternately irradiate, this reversible process repeatability are high.This implementation
The Ba of example preparation0.995Ti4O9:0.005Tm3+Photochromic material after 254nm ultraviolet excitation, color by white gradually
Become grey black, color is gradually recovered again as original white after sunlight irradiates.
Embodiment as previously discussed is some embodiments of the present invention, but embodiments of the present invention are not limited in
This, other any various modifications done without departing from spirit of the invention and basic principle, simplification, improvement, modification and simple
Combination and displacement belong within the scope of the present invention.
Claims (7)
1. a kind of application of titanate material in ability of reverse photochromism product, which is characterized in that use ultraviolet light titanate
It is irradiated or is heat-treated with sunlight again after material；
The chemical formula of the titanate material is Ba1-xTi4O9:xRe；
Wherein, Re is rare earth element, one in Y, La, Ce, Pr, Nd, Sm, Gd, Tb, Dy, Ho, Er, Tm, Eu, Yb and Lu
Kind is a variety of；
X is the doping mole of Re, 0≤x≤0.1；
The titanate material mixes the preparation method comprises the following steps: will contain Ba compound, compound containing Ti and compound containing Re, is burnt
Knot, obtains the titanate material；
The molar ratio of Ba, Ti and Re are (1-x): 4:x in the compound containing Ba, compound containing Ti and compound containing Re；0≤x
≤0.1。
2. application according to claim 1, which is characterized in that the compound containing Ba is selected from the nitre of the carbonate of Ba, Ba
One of oxide of hydrochlorate and Ba is a variety of；
The compound containing Ti is selected from one of nitrate of the oxide of Ti, the carbonate of Ti and Ti or a variety of；
The compound containing Re is selected from the oxide of Re and/or the nitrate of Re.
3. application according to claim 1, which is characterized in that the temperature of the sintering is 1100~1400 DEG C.
4. application according to claim 1, which is characterized in that the time of the sintering is 3~6h.
5. application according to claim 1, which is characterized in that the atmosphere of the sintering is air atmosphere.
6. application according to claim 1, which is characterized in that before the sintering further include pre-burning；
The temperature of the pre-burning is 500~600 DEG C.
7. application according to claim 6, which is characterized in that the soaking time of the pre-burning is 2~3h.
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| CN110467456A (en) * | 2019-09-16 | 2019-11-19 | 桂林电子科技大学 | A kind of material and preparation method thereof with reversible thermo-optic modulation characteristic |
| CN115215641A (en) * | 2022-08-10 | 2022-10-21 | 松山湖材料实验室 | Photochromic ceramic, preparation method thereof and optical device |
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| "Synthesis of BaTi4O9 ceramics by reaction-sintering process";Y. Liou et al.，;《Materials Research Bulletin》;20051231;第40卷(第9期);第1483-1489页 |
| Luminescence properties of red-emitting praseodymium-activated BaTi4O9 phosphor;L. Tian et al.，;《Journal of Luminescence》;20090305;第129卷(第8期);第797-800页 |
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